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By H. C. Ko

As part of the Bureau of Mines effort to provide thermodynamic data for the advancement of mineral technology, the standard enthalpies of formation for ZnO?2ZnSO4 and COS04-6H20 were determined by HC1 acid solution calorimetry. The values are -550.31 ±0.28 and -641.33 ±0.15 kcal/mot, respectively.

Jan 1, 1982

By E. Morrice

As part of its efforts to maximize process efficiency and decrease energy requirements in mineral processes, the Federal Bureau of Mines has investigated methods for beneficiating bastnäsite ores from Mountain Pass, Calif. The results of a bench-scale study on the flotation of bastnäsite ore are presented. Flotation at a pulp temperature of 40° to 45°C yielded a cleaner concentrate containing 58.7 pct RE203 at a rare-earth recovery of 67 pct. These results are comparable to those reported for the commercial beneficiation method in which the pulp is heated to boiling before flotation. An attempt was also made to recover a barite flotation concentrate from the bastnäsite rougher tailing. Concentrates containing only 70 pct barite were obtained.

Jan 1, 1982

By H. H. Dewing

The Bureau of Mines constructed a process research unit (PRU) to demonstrate new technology for extracting zinc from sphalerite concentrates. Up to 9 kg/hr of sphalerite (ZnS) concentrate was reacted at ambient pressure in the PRU with 80 pct sulfuric acid at 160° to 180° C to produce zinc sulfate and elemental sulfur. The PRU consisted of a three-stage glass reactor system: a 4-liter premix stage in which feed was slurried with 78 to 82 pct H2S04, a 40-liter stirred reactor, and a ISO-liter settling stage in which high reaction conversions were effected and excess H2S04 for recycle was separated from insoluble ZnS04 and sulfur. Evolution of sulfur-containing gases was minimized by sub-surface addition of acid feed slurry to the stirred reactor and by exclusion of air from the reactor to prevent the oxidation of elemental sulfur. Conversion of zinc to zinc sulfate averaged over 99 pct at the optimum acid concentration of 80 pct. Total sulfur losses (primarily S02) were less than 2 pct of the sulfur in the sphalerite. Elemental sulfur remained in the insoluble portion of the settled reactor product after leaching with simulated spent zinc electrolyte containing sulfuric acid. The sulfur residue contained 75 to 89 pct sulfur. Neutral zinc sulfate, required for zinc electrowinning processes, was separated from the sulfuric acid leach solution by crystallization at -15° C as zinc sulfate heptahydrate (ZnS04?7H20). The crystallization operation simultaneously effected a partial concentration of the recycled electrolyte solution by removing water.

Jan 1, 1982

By John P. Coughlin

Software techniques developed by the Bureau of Mines Denver Research Center for real-time microseismic data analysis are presented. These techniques focus on the simple acquisition of P-wave arrival times and their use in event location. The paper discusses in detail software techniques to separate microseismic events from mining noise such as drilling and from very large events such as rock bursts. Incorporation of these techniques has enhanced the reliability and accuracy of computer-based monitoring of microseismic activity in ongoing research by the Bureau.

Jan 1, 1982

By J. W. Walkiewicz

One of the objectives of the Bureau of Mines is to develop substitution technology for scarce materials. In accordance with this goal, alloys containing lanthanum, cobalt, copper, and magnesium were investigated for fabrication of rare-earth-cobalt (RE-Co) permanent magnets. A complete substitution of lanthanum for samarium and a partial substitution of copper for cobalt was accomplished. Magnets of La-Co and La-Co-Cu-Mg alloys were fabricated by powder metallurgy techniques and evaluated. A maximum intrinsic coercivity of 23.2 kOe was obtained with a La-Co-Cu-Mg alloy. In comparison, maximum values of 9.3 kOe and 11.6 kOe were obtained with La-Co and La-Co-Cu alloys, respectively. The substitution of copper and magnesium for part of the cobalt resulted in a large increase of intrinsic coercivity, similar to the results of Bureau research with mischmetal-Co-Cu-Mg alloys. Unlike the mischmetal-Co-Cu-Mg magnets, the La-Co-Cu-Mg magnets showed signs of physical deterioration on exposure to air. The effects of fabrication parameters on the magnetic properties of the La-Co-Cu-Mg alloys were also determined.

Jan 1, 1982

By A. D. Mah

To assist Bureau of Mines research in extractive metallurgy and to add to the thermodynamic data base useful to others, energy calculations were made for 63 reactions relating to investigations on the production of anhydrous aluminum chloride from chlorination of clay.

Jan 1, 1982

By William H. Pomroy

The Bureau of Mines, through a 4-year program of combined in-house and contract research, has developed the necessary hardware and software technology to provide rugged, reliable automatic fire protection for surface mining mobile equipment. One element of this program was a continuing effort to help foster rapid mining industry acceptance of the technology by keeping end user costs reasonable. This report is an analysis of the economic impact of surface mining mobile equipment fires and the cost benefit of utilizing automatic fire protection systems to abate these losses.

Jan 1, 1982

By Victor R. Spironello

The Bureau of Mines has conducted studies of the slags related to ferrous technology to evaluate experimentally acceptable substitutes for the auxiliary flux, mineral fluorspar, in steelmaking operations. Comparative heats were made in a 1/4-ton, pilot-scale, basic oxygen furnace (BOF) to evaluate a waste material known as "used potlining." Used pot lining is recovered from alumina reduction cells after its useful life and contains significant levels of fluorine and sodium in various compounds. This material in both lump and pelletized form provided adequately fluid slags, based on observations made during BOF operation. No adverse effects were found on furnace performance, metal and slag chemsitry, the strength of the steel produced, or the environment. Fluorine recovery in the slag was about the same as that obtained when using fluorspar, as were the losses to the scrubber water and solids. No difference was observed in furnace-refractory attack, as determined by the level of magnesia in the slag. The sodium recovered in the slag apparently also contributed to fluidity, since the fluorine input was at about two-thirds that of the fluorspar. Used potlining was determined experimentally to be a satisfactory substitute for fluorspar in basic oxygen steelmaking.

Jan 1, 1982

By David M. Hyman

The Bureau of Mines has developed two experimental designs for deter- mining the volumes and relative proportions of the various gas species, particularly methane (CH4), occluded in rock salt. To date, the rock salt samples analyzed have been relatively small (400- to 1,000-gram) grab samples from Louisiana Gulf Coast domal salt mines. The results obtained are comparable to results in Polish domal salt mines, in terms of occluded gas volumes per mass of rock salt. The notable difference between the Louisiana and Polish occluded gas mixtures is in the relative proportions of the individual gas species. The two methods used by the Bureau are ballmill crushing and dissolution. Of the two, the dissolution method appears to be more versatile because it can be performed in situ. The relevance and applicability of data on the occluded gas contents of rock salt are dependent on sample size, sample collection method, geologic context of the sample, and the correlation with gas emissions that occur as a result of mining-induced fractures and pressure differentials.

Jan 1, 1982

By Richard J. Mainiero

The Bureau of Mines conducted research to evaluate the optimum design for a rock-breaking explosive charge that could be fired unconfined in a gassy or dusty coal mine without the danger of igniting the flammable atmosphere. Charges of various shapes, with and without cavities, were tested in a gallery using 3-by 3-by l-ft concrete blocks as simulated boulders. For these tests the optimum charge, in terms of cost, weight, and convenience in handling, consisted of a flat l-1/2-lb charge of permissible explosive seven-eighths of an inch thick and 7 in in diameter encased in a l/2-in thick layer of fine salt (NaCI). This work demonstrated that it should be possible to produce an inexpensive explosive rock-breaker charge that would be safe to use in underground coal mines.

Jan 1, 1982

By Seth C. Schaefer

The Bureau of Mines investigated thermodynamic properties of Mn304 (manganomanganic oxide) and Mn203 (manganese sesquioxide). The standard Gibbs energies of formation (?Gf°) of Mn304 and Mn203 from their lower oxides were determined with high-temperature galvanic cells using stabilized Zr02 (zirconia) as the electrolyte. Potential measurements were obtained for the cell Pt, MnO, Mn304//Zr0 2//02(g, 0.0112 atm), Pt, with the overall cell reaction 6Mn0(c) + 02(g, 0.0112 atm) = 2Mn304(c), where- 02 refers to indicated partial pressure of oxygen at the reference electrode. Similar measurements were obtained for the cell Pt, Mn304, Mn203//ZrO2//02(g, 0.0115 atm), Pt, with the overall cell reaction 4Mn304(c) + 02(g, 0.0115 atm) = 6Mn203(c). Equilibrium oxygen pressures for the Mn0-Mn304-02 and Mn304-Mn203-02 systems were measured and may be expressed for the respective systems as [23,400 109 P02 T + 11.91 (764.9 - 1,208.6 K) and log p02 = - 11,957 + 9.66 T (968.6 - 1,208.2 K),] where pressure (p02) is in atmospheres and temperature (T) is in kelvins. Standard thermodynamic properties of Mn304 and Mn203 were derived from these measurements and auxiliary thermodynamic data from the literature.

Jan 1, 1982

By Jack C. White

As part of an investigation of the production of alumina by the nitric acid leaching of kaolinitic clay, the Bureau of Mines designed, built, and tested a fluidized-bed system for the calcination of aluminum nitrate nonahydrate to alumina, while recovering nitric acid. The calciner consisted of an 8-in-square by 36-in-tall vessel containing 18 in of fluidized solids. Molten aluminum nitrate, sprayed directly into the fluidized solids, formed sandy, granular alumina by growth of successive layers on fluidized particles. Solids were fluidized in a dense bed at temperatures of 250° to 500° C with steam, air, or mixtures thereof. Decomposition of nitrate ranged from 4 to 10 pet during single-pass steam or air fluidization, respectively. Alumina dust losses and low throughput are significant unsolved problem areas.

Jan 1, 1982

By Stephen D. Cramer

The solubility of methane, carbon dioxide, and oxygen was measured in brines at temperatures from 0° to 300° as part of Federal Bureau of Mines research on the corrosion of metals in high-temperature geothermal and mineral processing environments. Solubilities were measured by the technique of extracting pure gas, dissolved at pressures where Henry's law was applicable, from known volumes of brine. The results were smoothed with respect to temperature. The solubility, expressed in terms of the Henry's law constant, reaches a maximum at temperatures ranging from 60° to 100° C for methane and oxygen, and from 160° to 170° C for carbon dioxide. The Henry's law constant increases, that is, gases are salted out of the brines, in the presence of dissolved salts. Salting-out coefficients are strongly dependent upon temperature. The temperature dependence of the Henry's law constant for geothermal brines is different from that for sodium chloride brines owing to the more complex chemistry of the geothermal brines. The solubility of oxygen and carbon dioxide in brines exposed to air saturated with water vapor and at a total pressure of 760 mm Hg is reported for temperatures from 0° C to the normal boiling point.

Jan 1, 1982

By Martin Hertzberg

The Bureau of Mines 8-liter flammability system was used to study the effectiveness of a variety of powdered inhibitors in preventing the propagation of explosions of coal dust or methane in air. Over 35 different chemical additives were evaluated against Pittsburgh seam pulverized coal. The least effective inhibitors were the carbonates, which required mass additions in the range of two to three parts inhibitor to one part of coal dust in order to prevent propagation. The most effective inhibitors were the derivatives of ammonium phosphate, which were effective quenching agents at additions of only one part inhibitor to four parts of coal dust. Alkali halide powders were of intermediate effectiveness. These laboratory-scale results are in good agreement with full-scale mine experiments in all cases where detailed comparisons have been made. Data were also obtained for the effectiveness of several of the same powdered inhibitors against methane-air explosions. Their relative order of effectiveness and the concentration ranges required for quenching the gas explosion are comparable to those measured for coal dust explosions. Data are also presented for the effectiveness of N2 and CF3Br addition. Some preliminary data are also presented for powder addition to methane burner flames. Those data are compared with other burner data and evaluated in terms of their relevance to explosion tests.

Jan 1, 1982

By D. S. Burgess

About 100 tests of flammability were carried out with H2, CH4, and CO in mixtures with air using the Federal Bureau of Mines 12-ft-diameter spherical pressure vessel as an explosion test chamber. The LeChatelier approximation gave slightly conservative estimates of the limits of downward flame propagation (onset of significant pressure rise) using the following measured values for the individual gases, in percent: H2, 8.5; CH4, 5.25; CO, 13.0. No justification could be offered for using the LeChatelier law for upward flame propagation limits and indeed reported data suggest that calculated values would not be conservative. The observed upward limit for methane-air mixtures (4.85 pct) was less than the widely accepted lean limit for this fuel; those for lean hydrogen-air mixtures and carbon monoxide-air mixtures did not differ from the lowest accepted values. Diffusional effects on the propagation of single, binary, and ternary fuel mixtures are discussed.

Jan 1, 1982

By J. M. Stuve

A novel calorimetric solution technique, recently developed at the Bureau of Mines, was tested using synthetic samples of chalcocite (CU2S) and covellite (CuS). The solution of these refractory sulfides was accomplished by oxidation with bromine in a moderately acidic, aqueous solution. The resulting values for the standard enthalpies of formation (?Hf°, 298.15) for CU2S(c) and CuS(c) were -18.1 ±1.1 kcal/mol and -13.3 ±1.1 kcal/mol, respectively. These values are in good agreement with published formation values derived from other methods of physicochemical measurement.

Jan 1, 1982

By John L. Schaller

The Bureau of Mines, U.S. Department of the Interior, has investigated the extraction of alumina from domestic kaolin clay by leaching with boiling 26 wt-pct hydrochloric acid. Acid leaching of crushed calcined kaolin feed yields slurries that are slow settling and difficult to filter because of the presence of fine particles generated in crushing, calcining, and leaching. Laboratory research showed that tumbling and moistening crushed raw kaolin on a pelletizing disk caused the fines to agglomerate on the surfaces of the larger particles, while the sharp edges and corners of the larger particles were rounded off. Minus 16-mesh crushed raw kaolin was misted on a 36-in-diam, 8-in-deep pelletizing disk at rates of 175 to 250 lb/hr, and was calcined in either a rotary or a fluidized-bed calciner; negligible degradation occurred. The physical properties of the misted calcined kaolin were evaluated in the leaching system of the clay-hydrochloric acid miniplant. Only minor attrition occurred during leaching, and the slurry was readily filtered on a continuous belt filter.

Jan 1, 1982

By Masami Hayashi

The Bureau of Mines conducted laboratory studies to investigate methods for desilicating sodium aluminate solution derived from leaching a limestone-anorthosite sinter with 10-pct Na2C03 solution. Desilication tests were made at atmospheric pressure to determine the effects of time and additions of lime and desilication residues. A two-stage, countercurrent desilication procedure was developed to reduce the Si02 content sufficiently to meet specifications for cell-grade A1203. Both stages were conducted at boiling temperatures at atmospheric pressure. Reagent lime was charged as desilication seed to the partially desilicated solution in the second stage, and a product (desilication residue) precipitated by the lime addition was charged to the freshly leached solution in the first stage. Average A1203 loss in the desilication circuit was 5.8 pct, and the product solution contained less than 0.04 g/l Si02. Complete precipitation of A1203 by carbonation resulted in a hydrate containing less than 0.01 pct Si02. Calcination of this hydrate would produce A1203 meeting the 0.015 pct Si02 specification for cell-grade material.

Jan 1, 1982

By V. E. Edlund

As part of a research program for recovering alumina from domestic nonbauxitic resources, the Bureau of Mines investigated a lime-sinter, caustic leach technology for anorthosite. This report discusses the unit operations--feed preparation, sintering, and leaching. Acceptable pellets for the bench-scale sintering studies were prepared from mixtures of minus 200-mesh anorthosite and limestone using water alone as the pelletizing agent. Heating pellets at 1,270° to 1,360° C for periods of 0.5 to 2 hr, followed by a 15-min soaking period at 700° C and cooling to room temperature, produced a sinter that dusted to more than 90 pct minus 65 mesh. The weight ratio of limestone to anorthnsite was critical in producing sinter exhibiting good dusting and leaching characteristics. A ratio of 2.0 was optimum for the bulk samples of anorthosite and limestone used in this research. Leach solutions from lower ratio sinters were unstable; gelation became progressively more severe with higher ratio sinters. Leaching the dusted sinter with 10-pct Na2CO3 at 60° C extracted 85 to 90 pct of the alumina in a product solution containing about 50 g/l A1203. Leach residue in contact with pregnant solution tended to set up as a rigid gel as a result of cementation, comp action, and gelation. The presence of a calcium-sodium zeolite [(Cn,Na2)6?(Al2Si04)12?27-3OH20] in the ungelled residues seemed to be the main difference between gelled and ungelled residues.

Jan 1, 1982

By R. Emmett Hughlett

The Bureau of Mines has developed a statistical approach to the laboratory evaluation of response bias and precision in gas detectors. The techniques described employ a computerized analysis and a new method of data presentation called composite graphing. The underlying theory, its practical application to the data, and the experimental equipment and procedure are described.

Jan 1, 1982